Hydrazine → HCID 178496297, 화합물

HRID 1492986

반응식

HRID 1492986 반응식
[NH2:1][NH2:2].[H-].[Na+].[CH3:5][C:6]([C:9]1[CH:10]=[C:11]([CH:14]=[C:15]([C:24]([CH3:27])([CH3:26])[CH3:25])[C:16]=1[O:17][CH2:18][O:19][CH2:20][CH2:21][O:22][CH3:23])[C:12]#[N:13])([CH3:8])[CH3:7].C(=O)(O)[O-].[Na+]>O1CCCC1.O>[CH3:8][C:6]([C:9]1[CH:10]=[C:11]([C:12]([NH:1][NH2:2])=[NH:13])[CH:14]=[C:15]([C:24]([CH3:27])([CH3:26])[CH3:25])[C:16]=1[O:17][CH2:18][O:19][CH2:20][CH2:21][O:22][CH3:23])([CH3:5])[CH3:7]

참가 물질

7

반응물 4

HCID 9321HydrazineHCID 24758Sodium hydrideHCID 516892Sodium BicarbonateHCID 100416433,5-Bis(1,1-dimethylethyl)-4-[(2-methoxyethoxy)methoxy]benzonitrile

생성물 1

HCID 178496297HCID 178496297, 화합물수율 67%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
0 °C

실험 절차

97% anhydrous hydrazine (4.8 g, 0.151 mole) is added dropwise to a stirred 0° C. suspension of sodium hydride (2.8 g of a 60% dispersion in mineral oil, 0.071 mol) in tetrahydrofuran (70 ml) under nitrogen. After 90 minutes, a solution of 3,5-bis(1,1-dimethylethyl)-4-[(2-methoxyethoxy)methoxy]benzonitrile (6.7 g, 0.021 mole) in tetrahydrofuran (15 ml) is added dropwise. After stirring two hours at 0° C., water (2.4 ml) is added dropwise. The mixture is poured into cold, saturated aqueous sodium bicarbonate (20 ml). The product is extracted with a 1:1 ethyl acetate/ether mixture (60 ml). The organic layer is washed with saturated aqueous NaCl and dried over MgSO4. Filtration and concentration provided a solid which was recrystallized from ethyl acetate/hexane to give 4.9 g (7.3 g theor., 67%) of 3,5-bis(1,1-dimethylethyl)-4-[(2-methoxyethoxy)methoxy]benzene carboximidic acid hydrazide, mp 133° C.

후처리

  1. extractionThe product is extracted with a 1:1 ethyl acetate/ether mixture (60 ml)
  2. washThe organic layer is washed with saturated aqueous NaCl
  3. dry with materialdried over MgSO4
  4. filtrationFiltration and concentration
  5. customprovided a solid which
  6. customwas recrystallized from ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-db6d76dc90794e54b5cd91af134f132d
출처 데이터셋
uspto-grants-1994_12
특허 번호
US05376670

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